CN112730488B - Calibration method for measuring residual austenite in steel by X-ray diffraction method - Google Patents

Calibration method for measuring residual austenite in steel by X-ray diffraction method Download PDF

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CN112730488B
CN112730488B CN202110151899.7A CN202110151899A CN112730488B CN 112730488 B CN112730488 B CN 112730488B CN 202110151899 A CN202110151899 A CN 202110151899A CN 112730488 B CN112730488 B CN 112730488B
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sample
ray diffraction
residual austenite
steel
zero
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CN112730488A (en
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尤绍军
孙小东
王红伟
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Luoyang Bearing Group Co ltd
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Luoyang LYC Bearing Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/207Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/05Investigating materials by wave or particle radiation by diffraction, scatter or reflection
    • G01N2223/056Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/10Different kinds of radiation or particles
    • G01N2223/101Different kinds of radiation or particles electromagnetic radiation
    • G01N2223/1016X-ray
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/30Accessories, mechanical or electrical features
    • G01N2223/303Accessories, mechanical or electrical features calibrating, standardising
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/60Specific applications or type of materials
    • G01N2223/624Specific applications or type of materials steel, castings
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Crystallography & Structural Chemistry (AREA)
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Abstract

A calibration method for determining steel grade residual austenite by an X-ray diffraction method relates to the technical field of bearing heat treatment nondestructive testing, and comprises the following specific steps: step one: preparing a bearing steel No. 0 sample with zero retained austenite content; step two: obtaining a zero offset value A of the measuring equipment; detecting the prepared 0# sample with zero residual austenite content by using an X-ray diffraction device, and taking the obtained detection value A as a zero offset value; step three: detecting a sample to be detected by using the same X-ray diffraction equipment, wherein the residual austenite content Y=an actual measured value B-zero offset value A of the sample to be detected; the calibration method can correct the residual austenite content measured by an X-ray diffraction method, so that the measurement result is more accurate.

Description

Calibration method for measuring residual austenite in steel by X-ray diffraction method
Technical Field
The invention relates to the technical field of nondestructive testing of heat treatment of bearings, in particular to a calibration method for measuring steel grade residual austenite by an X-ray diffraction method.
Background
According to the diffraction principle of X rays, the cumulative intensity of X-ray diffraction lines of a certain phase is improved along with the increase of the relative content of the phase in a sample, and the content of residual austenite in steel is calculated by measuring the cumulative intensity of martensite phase and austenite phase diffraction lines of bearing steel, but equipment and calculation deviation generally exist in the measuring process, and the deviation is generally between 1 percent and 2 percent; the precision bearing, the rolling mill bearing and the wind driven bearing have lower requirements on the residual austenite content in steel, generally have the requirement of not more than 3 percent, cannot obtain accurate measurement results under the deviation, and need a calibration method to correct the measurement results so as to accurately obtain the residual austenite content of the sample.
Disclosure of Invention
In order to overcome the defects in the background art, the invention discloses a calibration method for determining the residual austenite of steel grade by an X-ray diffraction method, which can correct the content of the residual austenite determined by the X-ray diffraction method, so that the measurement result is more accurate.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
a calibration method for determining steel grade residual austenite by an X-ray diffraction method comprises the following specific steps:
step one: preparing a bearing steel No. 0 sample with zero retained austenite content; spheroidizing annealing is carried out on a high-carbon chromium bearing steel GCr15 or GCr15SiMn sample, and the high-carbon chromium bearing steel is firstly put into a heating furnace for heating at the temperature: 790 ℃ +/-10 ℃ and heat preservation time: 6-7 h; then opening a furnace cover to rapidly cool to 620+/-10 ℃; then heating to 720+/-10 ℃ along with the furnace, and preserving heat for 2-3 h; finally, the furnace is cooled to 600+/-10 ℃ and discharged.
Step two: obtaining a zero offset value A of the measuring equipment; and detecting the prepared 0# sample with the residual austenite content of zero by using an X-ray diffraction device, and taking the obtained detection value A as a zero offset value.
Step three: and detecting the sample to be detected by using the same X-ray diffraction equipment, wherein the residual austenite content Y=the actual measured value B-the zero offset value A of the sample to be detected.
Further, in the third step, the absolute value of the actual measurement value of the sample to be measured is less than 6%.
Further, when the absolute value of the actual measured value of the sample to be measured is more than or equal to 6%, the X-ray diffraction equipment is replaced, and calibration is carried out again.
Further, the sample to be measured is required to be the same as the material of the sample No. 0.
Further, the incubation time of the sample # 0 in the heating stage in step one was 6.5h.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
the calibration method for determining the residual austenite of the steel grade by using the X-ray diffraction method disclosed by the invention can be used for more accurately detecting the residual austenite content in steel tapping, solving the problem that the residual austenite content of bearing parts with low requirements on the residual austenite content of a precision bearing, a rolling mill bearing, a wind power bearing and the like cannot be accurately obtained by using the X-ray diffraction method, facilitating the provision of technical support for the optimization and adjustment of a heat treatment process and meeting the requirements of users.
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Detailed Description
The invention will be explained in detail by the following examples, which are not intended to limit the invention to the following examples, and the purpose of the invention is to protect all technical modifications within the scope of the invention:
embodiment one:
a calibration method for determining steel grade residual austenite by an X-ray diffraction method comprises the following specific steps:
step one: preparing a bearing steel No. 0 sample with zero retained austenite content; firstly, spheroidizing annealing is carried out on a high-carbon chromium bearing steel GCr15 or GCr15SiMn sample, and the high-carbon chromium bearing steel is firstly put into a heating furnace for heating at the temperature: 780 ℃, the heat preservation time is as follows: 6h; then opening a furnace cover to cool to 610 ℃; then heating to 710 ℃ along with the furnace, and preserving heat for 2 hours; finally, furnace cooling to 590 ℃ and discharging;
step two: obtaining a zero offset value A of the measuring equipment; detecting the prepared 0# sample with zero residual austenite content by using an X-ray diffraction device, and taking the obtained detection value A as a zero offset value;
step three: detecting a sample to be detected by using the same X-ray diffraction equipment, wherein the sample to be detected is required to be the same as the selected 0# sample in material, and the residual austenite content Y of the sample to be detected is equal to the actual measured value B-zero offset value A; in addition, in order to ensure more accurate calibration, in the third step, the absolute value of the actual measured value of the sample to be measured needs to be less than 6%, and generally, according to the deviation requirement, the austenite of the sample to be measured is only less than 6%, so that the method has the significance of calibration; when the absolute value of the actual measured value of the sample to be measured is more than or equal to 6%, the proper X-ray diffraction equipment can be selected to be replaced based on the uncertainty of the measurement deviation of the X-ray diffraction equipment, and calibration can be carried out again.
Embodiment two:
the difference from the first embodiment is in the first step:
step one: preparing a bearing steel No. 0 sample with zero retained austenite content; spheroidizing annealing is carried out on a high-carbon chromium bearing steel GCr15 or GCr15SiMn sample, and the high-carbon chromium bearing steel is firstly put into a heating furnace for heating at the temperature: 790 ℃, heat preservation time: 6.5h; then opening a furnace cover to cool to 620 ℃; then heating to 720 ℃ along with the furnace, and preserving heat for 2.5h; finally, the furnace is cooled to 600 ℃ and discharged.
Embodiment III:
the difference from the first embodiment is in the first step:
step one: preparing a bearing steel No. 0 sample with zero retained austenite content; spheroidizing annealing is carried out on a high-carbon chromium bearing steel GCr15 or GCr15SiMn sample, and the high-carbon chromium bearing steel is firstly put into a heating furnace for heating at the temperature: 800 ℃, and the heat preservation time is as follows: 7h; then opening a furnace cover to cool to 630 ℃; then heating to 730 ℃ along with the furnace, and preserving heat for 3h; finally, the furnace is cooled to 610 ℃ and discharged.
Residual austenite content%
The invention is not described in detail in the prior art.

Claims (5)

1. A calibration method for measuring residual austenite in steel by an X-ray diffraction method is characterized by comprising the following steps of: comprises the following specific steps:
step one: preparing a bearing steel No. 0 sample with zero retained austenite content;
spheroidizing annealing is carried out on a high-carbon chromium bearing steel GCr15 or GCr15SiMn sample, and the high-carbon chromium bearing steel is firstly put into a heating furnace for heating at the temperature: 790 ℃ +/-10 ℃ and heat preservation time: 6-7 h; then opening a furnace cover to rapidly cool to 620+/-10 ℃; then heating to 720+/-10 ℃ along with the furnace, and preserving heat for 2-3 h; finally, furnace cooling to 600+/-10 ℃ and discharging;
step two: obtaining a zero offset value A of the measuring equipment; detecting the prepared 0# sample with zero residual austenite content by using an X-ray diffraction device, and taking the obtained detection value A as a zero offset value;
step three: and detecting the sample to be detected by using the same X-ray diffraction equipment, wherein the residual austenite content Y=the actual measured value B-the zero offset value A of the sample to be detected.
2. The calibration method for determining the residual austenite of the steel grade by using the X-ray diffraction method as set forth in claim 1, wherein the method comprises the following steps: in the third step, the absolute value of the actual measured value of the sample to be measured is less than 6%.
3. The calibration method for determining the residual austenite of the steel grade by using the X-ray diffraction method as claimed in claim 2, wherein the method comprises the following steps of: when the absolute value of the actual measured value of the sample to be measured is more than or equal to 6%, the X-ray diffraction equipment is replaced, and calibration is carried out again.
4. The calibration method for determining the residual austenite of the steel grade by using the X-ray diffraction method as set forth in claim 1, wherein the method comprises the following steps: the sample to be measured is required to be the same as the material of the No. 0 sample.
5. The calibration method for determining the residual austenite of the steel grade by using the X-ray diffraction method as set forth in claim 1, wherein the method comprises the following steps: in the first step, the incubation time of the sample # 0 in the heating stage was 6.5 hours.
CN202110151899.7A 2021-02-04 2021-02-04 Calibration method for measuring residual austenite in steel by X-ray diffraction method Active CN112730488B (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS563623A (en) * 1979-06-19 1981-01-14 Kawasaki Steel Corp On-line measuring method of austenite contained in rolled steel sheet
US5148458A (en) * 1990-01-18 1992-09-15 Clayton Ruud Method and apparatus for simultaneous phase composition and residual stress measurement by x-ray diffraction
CN101446561A (en) * 2008-10-17 2009-06-03 武汉钢铁(集团)公司 Method for quantitatively measuring remaining austenite in steel by X-ray diffraction polar diagram data
CN102135506A (en) * 2010-01-26 2011-07-27 宝山钢铁股份有限公司 Method for detecting residual austenite in steel plate on line
CN103604821A (en) * 2013-11-27 2014-02-26 南京钢铁股份有限公司 Method for measuring austenite content of steel
JP2016194158A (en) * 2015-04-01 2016-11-17 新日鐵住金株式会社 Hot rolled steel sheet and manufacturing method therefor
CN106896124A (en) * 2017-04-24 2017-06-27 上海应用技术大学 The assay method of corresponding residual austenite content in a kind of bearing steel material heat treatment process

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS563623A (en) * 1979-06-19 1981-01-14 Kawasaki Steel Corp On-line measuring method of austenite contained in rolled steel sheet
US5148458A (en) * 1990-01-18 1992-09-15 Clayton Ruud Method and apparatus for simultaneous phase composition and residual stress measurement by x-ray diffraction
CN101446561A (en) * 2008-10-17 2009-06-03 武汉钢铁(集团)公司 Method for quantitatively measuring remaining austenite in steel by X-ray diffraction polar diagram data
CN102135506A (en) * 2010-01-26 2011-07-27 宝山钢铁股份有限公司 Method for detecting residual austenite in steel plate on line
CN103604821A (en) * 2013-11-27 2014-02-26 南京钢铁股份有限公司 Method for measuring austenite content of steel
JP2016194158A (en) * 2015-04-01 2016-11-17 新日鐵住金株式会社 Hot rolled steel sheet and manufacturing method therefor
CN106896124A (en) * 2017-04-24 2017-06-27 上海应用技术大学 The assay method of corresponding residual austenite content in a kind of bearing steel material heat treatment process

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